CN105536779A - Preparation method of Pd/TiO2 nanowire catalyst, prepared catalyst and application thereof - Google Patents
Preparation method of Pd/TiO2 nanowire catalyst, prepared catalyst and application thereof Download PDFInfo
- Publication number
- CN105536779A CN105536779A CN201511031991.0A CN201511031991A CN105536779A CN 105536779 A CN105536779 A CN 105536779A CN 201511031991 A CN201511031991 A CN 201511031991A CN 105536779 A CN105536779 A CN 105536779A
- Authority
- CN
- China
- Prior art keywords
- tio
- nano
- catalyst
- preparation
- wire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 56
- 239000002070 nanowire Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 20
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 239000007791 liquid phase Substances 0.000 claims abstract description 8
- 241000723346 Cinnamomum camphora Species 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 230000004044 response Effects 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract 3
- 239000000203 mixture Substances 0.000 abstract 2
- 239000012696 Pd precursors Substances 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical compound O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 36
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 15
- 229960004217 benzyl alcohol Drugs 0.000 description 6
- 235000019445 benzyl alcohol Nutrition 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000011943 nanocatalyst Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002940 palladium Chemical class 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/40—
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
- C07C45/38—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a Pd/TiO2 nanowire catalyst, the prepared catalyst and application thereof. The preparation method of the Pd/TiO2 nanowire catalyst includes the following steps that 1, TiO2 powder is added to a NaOH water solution, after the mixture is fully stirred, the mixed solution is transferred into a hydrothermal reaction kettle, a hydrothermal reaction is conducted for 36-48 hours at the temperature of 150-200 DEG C, acid cleaning, water cleaning, drying and baking at the temperature of 300-1000 DEG C are conducted, and finally a one-dimension of TiO2 nanowire carrier is obtained; 2, cinnamomum camphora plant leaves are dried in the sun and crushed, water is added, the mixture is stirred for 1-4 hours and then filtered, filtrate A is obtained, a Pd precursor is added to the filtrate A, stirring is conducted for 1-3 hours at the temperature of 50-90 DEG C, and a solution B is obtained; 3, the one-dimension of TiO2 nanowire carrier is added to the solution B, stirring is conducted for 1-3 hours, then filtering, water cleaning and drying are conducted, and the powder-shaped Pd/TiO2 nanowire catalyst can be obtained. The Pd/TiO2 nanowire catalyst is applied to a reaction for preparing benzaldehyde through benzaldehyde solvent-free liquid-phase oxidation and has good catalytic activity.
Description
Technical field
The present invention relates to a kind of Pd/TiO
2the preparation method of nano-wire catalyst, obtained Pd/TiO
2nano-wire catalyst and the application of this catalyst in benzyl alcohol oxidation reaction.
Background technology
Benzaldehyde is the important source material of medicine, dyestuff, spices and Resin Industry.There is environmental pollution in the method for current industrial production benzaldehyde, product difficulty is separated, and particularly contains the problems such as chlorine element in product.The chlorine element contained in benzaldehyde product limits its application industrially to a certain extent.It is predicted, the market demand of China's benzaldehyde in this year will reach 300,000 tons, and wherein the demand of " without chlorine " benzaldehyde accounts for half, and along with benzaldehyde demand increases fast, domestic will exist huge breach.Therefore, benzaldehyde " green " production technology of research and development technology good economy performance has become the study hotspot in this field.At present, phenmethylol liquid phase oxidation is due to technique is simple, advantages of environment protection has become production " without chlorine " benzaldehyde an environmental protection technique (ACSSustainableChem. & Eng., 2014,2,1752-1759).The catalyst of phenmethylol liquid phase oxidation mainly comprises loaded noble metal catalyst, supported non-precious metal catalyst (Cu, Fe etc.), loaded by heteropoly acid type catalyst etc., wherein the highest with the activity of noble metal catalyst, especially Supported Pd-Catalyst.
Carrier for load P d nano particle has a lot, as MgO, TS-1, SiO
2deng, but the interaction that there is itself and Pd nano particle is more weak, and in roasting or course of reaction, Pd nano particle easily sinters, and catalyst recovery utilizes the problems such as difficult.In recent years, one dimension TiO
2nano material is more and more subject to the attention of researcher due to the structure of its uniqueness.Zhang etc. (ApplCatalB-Environ, 2014,150,544-553) research finds TiO
2nanowire supported Fe
2o
3catalyst surface metal loss rate is lower, shows better Fenton catalytic performance.Wang etc. (Nanoscale, 2013,5,9739-9746) research finds one dimension TiO
2when in nano material, rutile and anatase two kinds of crystal formations coexist, the Au nanocatalyst of its load shows excellent performance to dye wastewater degradation.Known from analysis above, one dimension TiO
2structure (pattern and the crystal formation) catalytic performance to the metal nano catalyst of its load of nano material has a significant impact.Therefore, for Problems existing in current benzyl alcohol oxidation reaction, the present invention proposes to utilize one dimension TiO
2nano wire prepares the conception of Pd catalyst as carrier, and be oxidized for catalytic phenylmethanol, wherein Pd nano particle is by preparing using plant biomass extract as reducing agent, to expect to obtain high activity, the solvent-free liquid-phase oxidation catalyst of phenmethylol that is selective and stability.At present, about one dimension TiO
2nanowire supported Pd nanocatalyst biological reducing preparation and benzyl alcohol oxidation reaction in application also do not have correlative study to report.
Summary of the invention
First object of the present invention aims to provide a kind of Pd/TiO
2the preparation method of nano-wire catalyst, utilizes one dimension TiO
2nano wire carrys out the standby Pd nano particle of load biological reducing legal system as carrier, has that cost is low, simple to operate, the feature of environmental protection.
Second object of the present invention is to provide obtained Pd/TiO
2the application in the reaction of benzaldehyde prepared by nano-wire catalyst and this catalyst in the solvent-free liquid phase oxidation of phenmethylol, have high activity, high selectivity and be easy to the features such as recycling.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Pd/TiO
2the preparation method of nano-wire catalyst, comprises the steps:
1) by TiO
2powder joins in the NaOH aqueous solution, moves on in hydrothermal reaction kettle after fully stirring by mixed solution, at the Water Under thermal response 36 ~ 48h of 150 ~ 200 DEG C, through overpickling, washing, drying and 300-1000 DEG C roasting process, and final acquisition one dimension TiO
2nano wire carrier;
2) fragrant camphor tree plant leaves is dried, pulverizes, filter after the stirring 1 ~ 4h that adds water, obtain filtrate A, add Pd presoma toward filtrate A, under the condition of 50 ~ 90 DEG C, stir 1 ~ 3h, obtain solution B;
3) by one dimension TiO
2nano wire carrier joins in solution B, and filtration after stirring 1 ~ 3h, washing, drying, can obtain pulverous Pd/TiO
2nano-wire catalyst.
Further, step 1) in, TiO
2the preferred nanoscale TiO of powder
2powder, such as P25 type TiO
2powder.
Further, step 1) in, roasting time is 2 ~ 4h, preferred 4h.
Further, step 1) in, sintering temperature is preferably 450 ~ 600 DEG C, is more preferably 450 DEG C.
Further, step 1) in, described pickling adopts hydrochloric acid, sulfuric acid or nitric acid.
Further, step 2) in, the volume that adds of water counts 50-200mL/g with the quality of fragrant camphor tree plant leaves, is preferably 100mL/g.
Further, the preferred soluble palladium salt of described Pd presoma, as palladium nitrate.The molar concentration preferably making wherein Pd after adding Pd presoma in filtrate A is 0.25-1mM, is more preferably 0.5mM.
Step 3) in, those skilled in the art can determine one dimension TiO according to the actual needs of Pd load capacity
2the addition of nano wire carrier, generally makes Pd/TiO
2in nano-wire catalyst, Pd load capacity is 0.25 ~ 1%, and preferably 1%.
The present invention further provides obtained Pd/TiO
2nano-wire catalyst prepares the application in the reaction of benzaldehyde in the solvent-free liquid phase oxidation of phenmethylol.
Compared with prior art, beneficial effect of the present invention is: the present invention utilizes one dimension TiO first
2nano wire carrys out the standby Pd nano particle of load biological reducing legal system as carrier, and this preparation method has that cost is low, simple to operate, the feature of environmental protection.Obtained Pd/TiO
2nano-wire catalyst is used in the solvent-free liquid phase oxidation of phenmethylol and prepares in the reaction of benzaldehyde, has high activity, high selectivity and is easy to the features such as recycling.
Accompanying drawing explanation
Fig. 1 is that in transmission electron microscope (TEM) figure, Fig. 1 of the catalyst B of preparation in embodiment 2, scale is 100nm.
Detailed description of the invention
Below by embodiment, the present invention will be further described.
Embodiment 1
By the TiO of 1.5g
2(P25) powder joins in the NaOH aqueous solution, fully stirs 30min, and transfers in the hydrothermal reaction kettle of 200mL by solution, at the Water Under thermal response 48h of 200 DEG C, washes, washes through persalt, dry, and at 450 DEG C of roasting 4h, obtains one dimension TiO
2nano wire carrier, called after TiO
2(450).
Fragrant camphor tree plant leaves is dried, pulverized, gets 2g and add 200mL water, filter after stirring 2h, obtain filtrate A, the filtrate of getting 30mL adds the palladium nitrate aqueous solution of 200 microlitre 74mM, stirs 1.0h, obtains solution B, by appropriate TiO under the condition of 90 DEG C
2(450) nano wire carrier joins in solution B, makes the load capacity of Pd be 1wt%, and fully filtration after stirring 1h, washing, vacuum drying, obtain pulverous Pd/TiO
2nano-wire catalyst A.
Benzyl alcohol oxidation is reacted: add Pd/TiO in 50mL there-necked flask
2nano-wire catalyst 0.2g, and add 20mL phenmethylol, there-necked flask be placed in 90 DEG C of oil bath pan preheating 5min afterwards and reflux, the oxygen passing into 90mL/min afterwards starts reaction.Catalytic reaction the results are shown in Table 1.
Embodiment 2
By the TiO of 1.5g
2(P25) powder joins in the NaOH aqueous solution, fully stirs 30min, and transfers in the hydrothermal reaction kettle of 200mL by solution, at the Water Under thermal response 48h of 200 DEG C, washes, washes through persalt, dry, and at 600 DEG C of roasting 4h, obtains one dimension TiO
2nano wire carrier, called after TiO
2(600).
Solution B is prepared, by appropriate TiO according to the method for embodiment 1
2nano wire carrier joins in solution B, makes the load capacity of Pd be 1wt%, and fully filtration after stirring 1h, washing, vacuum drying, obtain pulverous Pd/TiO
2nano-wire catalyst B.Evaluating catalyst condition is with embodiment 1, and catalytic reaction the results are shown in Table 1.
Embodiment 3
By the TiO of 1.5g
2(P25) powder joins in the NaOH aqueous solution, fully stirs 30min, and transfers in the hydrothermal reaction kettle of 200mL by solution, at the Water Under thermal response 48h of 200 DEG C, washes, washes through persalt, dry, and at 700 DEG C of roasting 4h, obtains one dimension TiO
2nano wire carrier, called after TiO
2(700).
Solution B is prepared, by appropriate TiO according to the method for embodiment 1
2nano wire carrier joins in solution B, makes the load capacity of Pd be 1wt%, and fully filtration after stirring 1h, washing, vacuum drying, obtain pulverous Pd/TiO
2nano-wire catalyst C.Evaluating catalyst condition is with embodiment 1, and catalytic reaction the results are shown in Table 1.
Embodiment 4
By the TiO of 1.5g
2(P25) powder joins in the NaOH aqueous solution, fully stirs 30min, and transfers in the hydrothermal reaction kettle of 200mL by solution, at the Water Under thermal response 48h of 200 DEG C, washes, washes through persalt, dry, and at 800 DEG C of roasting 4h, obtains one dimension TiO
2nano wire carrier, called after TiO
2(800).
Solution B is prepared, by appropriate TiO according to the method for embodiment 1
2nano wire carrier joins in solution B, makes the load capacity of Pd be 1wt%, and fully filtration after stirring 1h, washing, vacuum drying, obtain pulverous Pd/TiO
2nano-wire catalyst D.Evaluating catalyst condition is with embodiment 1, and catalytic reaction the results are shown in Table 1.
Embodiment 5
By the TiO of 1.5g
2(P25) powder joins in the NaOH aqueous solution, fully stirs 30min, and transfers in the hydrothermal reaction kettle of 200mL by solution, at the Water Under thermal response 48h of 200 DEG C, wash through persalt, wash, dry, and at 1000 DEG C of roasting 4h, obtain one dimension TiO
2nano wire carrier, called after TiO
2(1000).
Solution B is prepared, by appropriate TiO according to the method for embodiment 1
2nano wire carrier joins in solution B, makes the load capacity of Pd be 1wt%, and fully filtration after stirring 1h, washing, vacuum drying, obtain pulverous Pd/TiO
2nano-wire catalyst E.Evaluating catalyst condition is with embodiment 1, and catalytic reaction the results are shown in Table 1.
Embodiment 6
Solution B is prepared, by the TiO of 0.5g according to the method for embodiment 1
2(P25) carrier joins in solution B, makes the load capacity of Pd be 1wt%, and fully filtration after stirring 1h, washing, vacuum drying, obtain pulverous Pd/TiO
2(P25) catalyst F (for contrast).Evaluating catalyst condition is with embodiment 1, and catalytic reaction the results are shown in Table 1.
Table 1Pd/TiO
2catalyst benzyl alcohol oxidation reactivity worth
Claims (10)
1. a Pd/TiO
2the preparation method of nano-wire catalyst, comprises the steps:
1) by TiO
2powder joins in the NaOH aqueous solution, moves on in hydrothermal reaction kettle after fully stirring by mixed solution, at the Water Under thermal response 36 ~ 48h of 150 ~ 200 DEG C, through overpickling, washing, drying and 300-1000 DEG C roasting process, and final acquisition one dimension TiO
2nano wire carrier;
2) fragrant camphor tree plant leaves is dried, pulverizes, filter after the stirring 1 ~ 4h that adds water, obtain filtrate A, add Pd presoma toward filtrate A, under the condition of 50 ~ 90 DEG C, stir 1 ~ 3h, obtain solution B;
3) by one dimension TiO
2nano wire carrier joins in solution B, and filtration after stirring 1 ~ 3h, washing, drying, can obtain pulverous Pd/TiO
2nano-wire catalyst.
2. Pd/TiO as claimed in claim 1
2the preparation method of nano-wire catalyst, is characterized in that: step 1) in, TiO
2powder is nanoscale TiO
2powder.
3. Pd/TiO as claimed in claim 1 or 2
2the preparation method of nano-wire catalyst, is characterized in that: step 1) in, roasting time is 2 ~ 4h.
4. Pd/TiO as claimed in claim 3
2the preparation method of nano-wire catalyst, is characterized in that: step 1) in, sintering temperature is 450 ~ 600 DEG C.
5. Pd/TiO as claimed in claim 4
2the preparation method of nano-wire catalyst, is characterized in that: sintering temperature is 450 DEG C, and roasting time is 4h.
6. Pd/TiO as claimed in claim 1 or 2
2the preparation method of nano-wire catalyst, is characterized in that: step 2) in, the volume that adds of water counts 50-200mL/g with the quality of fragrant camphor tree plant leaves, makes the molar concentration of wherein Pd be 0.25-1mM in filtrate A after adding Pd presoma.
7. Pd/TiO as claimed in claim 6
2the preparation method of nano-wire catalyst, is characterized in that: step 2) in, the volume that adds of water counts 100mL/g with the quality of fragrant camphor tree plant leaves, makes the molar concentration of wherein Pd be 0.5mM in filtrate A after adding Pd presoma.
8. Pd/TiO as claimed in claim 1 or 2
2the preparation method of nano-wire catalyst, is characterized in that: Pd/TiO
2in nano-wire catalyst, Pd load capacity is 0.25 ~ 1%.
9. the Pd/TiO that obtains of preparation method according to claim 1
2nano-wire catalyst.
10. Pd/TiO as claimed in claim 9
2nano-wire catalyst prepares the application in the reaction of benzaldehyde in the solvent-free liquid phase oxidation of phenmethylol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511031991.0A CN105536779B (en) | 2015-12-31 | 2015-12-31 | A kind of preparation method of Pd/TiO2 nano-wire catalyst, catalyst obtained and its application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511031991.0A CN105536779B (en) | 2015-12-31 | 2015-12-31 | A kind of preparation method of Pd/TiO2 nano-wire catalyst, catalyst obtained and its application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105536779A true CN105536779A (en) | 2016-05-04 |
| CN105536779B CN105536779B (en) | 2019-05-31 |
Family
ID=55816616
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511031991.0A Active CN105536779B (en) | 2015-12-31 | 2015-12-31 | A kind of preparation method of Pd/TiO2 nano-wire catalyst, catalyst obtained and its application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105536779B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107890867A (en) * | 2017-12-15 | 2018-04-10 | 浙江工业大学 | A kind of grey Pd/TiO2Nano wire photochemical catalyst and its preparation method and application |
| CN108325524A (en) * | 2018-02-08 | 2018-07-27 | 厦门大学 | A kind of preparation method of load type palladium catalyst for benzene catalysis oxidation |
| CN108772087A (en) * | 2018-05-17 | 2018-11-09 | 常州大学 | A kind of Supported Pd-Catalyst and preparation method thereof for benzyl alcohol oxidation synthesizing benzaldehyde under solvent-free system |
| CN109012662A (en) * | 2018-08-28 | 2018-12-18 | 浙江工业大学 | A kind of preparation method of photocatalysis benzyl alcohol oxidation catalyst |
| CN109331822A (en) * | 2018-11-16 | 2019-02-15 | 浙江工业大学 | A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof |
| CN109331819A (en) * | 2018-11-16 | 2019-02-15 | 浙江工业大学 | Titanium dioxide load-type Pt-Pd bimetallic photochemical catalyst and the preparation method and application thereof |
| CN115198285A (en) * | 2022-07-14 | 2022-10-18 | 西安泰金工业电化学技术有限公司 | Preparation method of noble metal powder catalyst for hydrogen production by water electrolysis |
| CN115672299A (en) * | 2021-07-30 | 2023-02-03 | 国家能源投资集团有限责任公司 | Titanium dioxide nanowire and preparation method thereof, denitration catalyst and preparation method thereof, and flue gas denitration method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4190605A (en) * | 1978-06-30 | 1980-02-26 | The Dow Chemical Company | Catalyst activation in oxidation process |
| CN1915835A (en) * | 2006-07-27 | 2007-02-21 | 北京先讯东泰科技有限公司 | Method for preparing Nano line of titania, and application of the prepared Nano line of titania |
| CN101219377A (en) * | 2008-01-11 | 2008-07-16 | 山东大学 | Precious metal/one-dimensional titanium dioxide nanostructure composite material and method for producing the same |
| CN102120184A (en) * | 2011-01-25 | 2011-07-13 | 中国科学院山西煤炭化学研究所 | Noble metal-carrying titanium dioxide catalyst and preparation method and use thereof |
| CN102600900A (en) * | 2012-01-20 | 2012-07-25 | 厦门大学 | Load-type gold-palladium bimetallic catalyst and preparation method thereof |
| CN104722302A (en) * | 2015-03-25 | 2015-06-24 | 浙江工业大学 | Acidified mixed crystal TiO2 nanowire loaded photocatalyst and preparation and application of photocatalyst |
-
2015
- 2015-12-31 CN CN201511031991.0A patent/CN105536779B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4190605A (en) * | 1978-06-30 | 1980-02-26 | The Dow Chemical Company | Catalyst activation in oxidation process |
| CN1915835A (en) * | 2006-07-27 | 2007-02-21 | 北京先讯东泰科技有限公司 | Method for preparing Nano line of titania, and application of the prepared Nano line of titania |
| CN101219377A (en) * | 2008-01-11 | 2008-07-16 | 山东大学 | Precious metal/one-dimensional titanium dioxide nanostructure composite material and method for producing the same |
| CN102120184A (en) * | 2011-01-25 | 2011-07-13 | 中国科学院山西煤炭化学研究所 | Noble metal-carrying titanium dioxide catalyst and preparation method and use thereof |
| CN102600900A (en) * | 2012-01-20 | 2012-07-25 | 厦门大学 | Load-type gold-palladium bimetallic catalyst and preparation method thereof |
| CN104722302A (en) * | 2015-03-25 | 2015-06-24 | 浙江工业大学 | Acidified mixed crystal TiO2 nanowire loaded photocatalyst and preparation and application of photocatalyst |
Non-Patent Citations (3)
| Title |
|---|
| PATCHARAPORN WEERACHAWANASAK ET AL: ""Surface functionalized TiO2 supported Pd catalysts for solvent-free selective oxidation of benzyl alcohol"", 《CATALYSIS TODAY》 * |
| ROBERT MENZEL ET AL: ""Impact of Hydrothermal Processing Conditions on High Aspect Ratio Titanate Nanostructures"", 《CHEMISTRY OF MATERIALS》 * |
| 纪镁铃等: ""生物还原法制备Pd/TiO2光催化剂"", 《化学反应工程与工艺》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107890867A (en) * | 2017-12-15 | 2018-04-10 | 浙江工业大学 | A kind of grey Pd/TiO2Nano wire photochemical catalyst and its preparation method and application |
| CN107890867B (en) * | 2017-12-15 | 2020-10-09 | 浙江工业大学 | Gray Pd/TiO2Nanowire photocatalyst and preparation method and application thereof |
| CN108325524A (en) * | 2018-02-08 | 2018-07-27 | 厦门大学 | A kind of preparation method of load type palladium catalyst for benzene catalysis oxidation |
| CN108772087A (en) * | 2018-05-17 | 2018-11-09 | 常州大学 | A kind of Supported Pd-Catalyst and preparation method thereof for benzyl alcohol oxidation synthesizing benzaldehyde under solvent-free system |
| CN108772087B (en) * | 2018-05-17 | 2021-04-27 | 常州大学 | Supported Pd catalyst for synthesizing benzaldehyde by oxidizing benzyl alcohol in solvent-free system and preparation method thereof |
| CN109012662A (en) * | 2018-08-28 | 2018-12-18 | 浙江工业大学 | A kind of preparation method of photocatalysis benzyl alcohol oxidation catalyst |
| CN109331822A (en) * | 2018-11-16 | 2019-02-15 | 浙江工业大学 | A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof |
| CN109331819A (en) * | 2018-11-16 | 2019-02-15 | 浙江工业大学 | Titanium dioxide load-type Pt-Pd bimetallic photochemical catalyst and the preparation method and application thereof |
| CN115672299A (en) * | 2021-07-30 | 2023-02-03 | 国家能源投资集团有限责任公司 | Titanium dioxide nanowire and preparation method thereof, denitration catalyst and preparation method thereof, and flue gas denitration method |
| CN115672299B (en) * | 2021-07-30 | 2024-04-30 | 国家能源投资集团有限责任公司 | Titanium dioxide nanowire and preparation method thereof, denitration catalyst and preparation method thereof, and flue gas denitration method |
| CN115198285A (en) * | 2022-07-14 | 2022-10-18 | 西安泰金工业电化学技术有限公司 | Preparation method of noble metal powder catalyst for hydrogen production by water electrolysis |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105536779B (en) | 2019-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105536779A (en) | Preparation method of Pd/TiO2 nanowire catalyst, prepared catalyst and application thereof | |
| CN106064087B (en) | A method of preparing VOCs catalyst for catalytic combustion | |
| CN106540694A (en) | Copper-based MOF materials prepare the Cu of porous carbon load2The method of O/Cu composites and its application | |
| CN107890867B (en) | Gray Pd/TiO2Nanowire photocatalyst and preparation method and application thereof | |
| EP2823900B1 (en) | Method for preparing solid nitrosyl ruthenium nitrate by using waste catalyst containing ruthenium | |
| CN109718806A (en) | A kind of monatomic catalyst of noble metal and its preparation method and application | |
| CN102161003B (en) | Preparation and application method of hydrazine-degrading catalyst | |
| CN103691431A (en) | Palladium carbon catalyst as well as preparation method and application thereof | |
| CN106975479B (en) | A kind of sea urchin shape CeO2-MnO2The preparation method of composite oxide catalysts | |
| CN103272601B (en) | A kind of preparation method of the catalyst for By Catalytic Hydrogenation of Nitrobenzene synthesis aniline | |
| CN103357424A (en) | Photocatalyst for selective oxidation of toluene and toluene derivatives | |
| CN104084194A (en) | Method for preparing high-selectivity platinum-carbon catalyst through vacuum impregnation | |
| CN103537310A (en) | Catalyst and method for preparing maleic anhydride by normal butane oxidization | |
| Liu et al. | A new cobalt metal–organic framework as a substrate for Pd nanoparticles applied in high-efficiency nitro phenol degradation and cinnamaldehyde hydrogenation | |
| CN103691434B (en) | A kind of metallic catalyst and preparation method and application | |
| CN109126777A (en) | A kind of method that platinum-containing waste catalyst prepares Pt/C catalyst | |
| CN103724174B (en) | A kind of method preparing pimelinketone | |
| CN102294252A (en) | Production method of solid super acidic catalyst S04<2->/Sb-SnO2 | |
| CN103055883A (en) | Supported nickel-based catalyst and its preparation method and use | |
| CN102633581A (en) | Application of nano titanium oxide mesoporous composite loaded platinum catalyst to catalytic hydrogenation | |
| CN110420662A (en) | It is a kind of can efficient degradation stalk cellulose at low temperature composite catalyzing material and the preparation method and application thereof | |
| CN104190435A (en) | Manganese-cobalt nanocrystalline catalyst for catalytic oxidation of methylbenzene as well as preparation method and application thereof | |
| CN102649062A (en) | Catalyst for production of hydroxyacetic acid ester by oxalate through hydrogenation | |
| CN104478664A (en) | Multiphase selective hydrogenation reaction method for cinnamyl aldehyde | |
| CN102259008B (en) | Solid acid catalyst for esterification reaction and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |